CN115501894A - 一种含氧空位AgIO3光催化剂及其制备方法与应用 - Google Patents
一种含氧空位AgIO3光催化剂及其制备方法与应用 Download PDFInfo
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Abstract
本发明属于无机半导体材料制备技术领域,具体涉及一种用于分解甲基橙的含氧空位AgIO3光催化剂及其制备方法。本发明以AgIO3为前驱体,经过在H2/N2混合气体下烧结,使AgIO3表面产生氧空位。在模拟太阳光照射下,烧结光催化剂对甲基橙的光催化降解性能相对于纯AgIO3得到很大提高,甲基橙的降解率最高可以达到77%。而且,性能最强的AgIO3‑Ov‑3催化剂能够有效降解盐酸四环素、盐酸金霉素、氧氟沙星、诺氟沙星、罗丹明B、磺胺异恶唑等有机污染物。AgIO3表面形成氧空位,拓宽了其可见光响应范围,并且有效地抑制了光生载流子复合,改善载流子迁移效率,从而提高了光催化效率。
Description
技术领域
本发明涉及无机半导体材料技术领域,尤其涉及一种含氧空位AgIO3光催化剂及其制备方法与应用。
背景技术
由于(IO3)-中的孤对电子,金属碘酸盐被广泛研究,这有利于层状结构的形成并使其极化。层状结构和极性在减少光诱导电子(e−)和空穴(h+)复合方面起到了非常重要的作用,从而大大提高了光催化活性。这些金属碘酸盐,在紫外光照射下对染料进行光解过程中的优异光催化性能表明,金属碘酸盐是一种很有前途的材料。此外,由于O 2p轨道和Ag 4d轨道的杂化,银基氧酸盐半导体也受到越来越多的关注,这将有助于提高VB(价带)。据报道,具有正交晶结构的AgIO3由于其宽禁带和高光激发电荷载体分离率,在紫外区域显示出良好的光催化性能。但由于碘酸银的带隙宽度较宽(约为3.59 eV),使其只能吸收在自然太阳光中占5%的紫外光,阻碍了碘酸银的实际应用。为了有效利用太阳光,因此需要对碘酸银进行改性研究,拓宽碘酸银的光谱响应范围。
构建氧空位是获得高性能可见光驱动光催化剂的可行方法,在光催化剂中引入表面氧空穴后,光响应波长范围扩大,紫外光活性大大提高。高浓度的表面氧空位有助于光生电子-空穴对的分离,提高光催化活性,这是因为表面氧缺陷态位于VB上方,部分与VB重叠,导致低态密度的价带最大值上升,VB变宽。此外,氧空位的产生也可以略微增加甲基橙上的吸附量,这是对增强光活性的补充。
发明内容
本发明旨在至少克服上述现有技术的缺点与不足其中之一,提供一种含氧空位AgIO3光催化剂及其制备方法与应用。本发明目的基于以下技术方案实现:
本发明目的的第一方面,提供了一种含氧空位AgIO3光催化剂的制备方法,包括以下步骤:
S1、将称好的AgIO3放置在坩埚中;
S2、将坩埚放入管式炉中加热升温,待温度升至300 ℃,保温30 min;
S3、反应结束后冷却,所得产物经过研磨后,得到AgIO3-Ov-3光催化剂。
本发明制备方法的原理为:将光催化剂作为自牺牲模板,对光催化剂进行烧结改性,能够开发高效、稳定、光吸收范围大、表面活性中心强的光催化剂,本发明的制备方法简单快捷,且绿色环保,可操作性强。
优选地,步骤S1中所述AgIO3的制备方法为:将硝酸银和五氧化二碘分别溶于水中,将五氧化二碘水溶液缓慢滴入硝酸银水溶液中,在室温下搅拌反应2 h,反应结束后,所得产物经离心、洗涤、烘干后,得到AgIO3。
优选地,所述硝酸银:五氧化二碘的摩尔比为2:1。
优选地,步骤S1中所述AgIO3的粒径为0.5~3 μm。
优选地,步骤S1中所述称量为0.2 g。
优选地,步骤S2中所述加热升温的升温速率为5 ℃/min。
优选地,步骤S2中所述保温时间为30 min。
优选地,步骤S3中所述冷却为自然冷却。
本发明目的的第二方面,提供了一种含氧空位AgIO3光催化剂,根据以上任一项所述的制备方法制得。
本发明目的的第三方面,提供了一种含氧空位AgIO3光催化剂在光催化降解有机染料方面的应用。
本发明可至少取得如下有益效果其中之一:
1)本发明以AgIO3为自牺牲模板,经过在H2/N2混合气体下烧结,使AgIO3表面产生氧空位。表面氧空位的生成有利于电子传导,有效降低了电子空穴的复合几率,同时减小了其禁带宽度扩大光吸收范围。在太阳光照射下,含氧空位AgIO3光催化剂对甲基橙的光催化降解性能相对于纯AgIO3得到很大提高,甲基橙的降解率最高可以达到77%。
2)本发明制备所得含氧空位AgIO3光催化剂,相比于单纯的AgIO3,既增强了电子的富集作用,还扩大了光吸收范围,提高了光的利用率,从而提高了光催化效果。
3)本发明制备所得含氧空位AgIO3光催化剂,相比于传统的金属氧化物半导体光催化剂,具有更优良的热稳定性、化学稳定性和电荷传递效率。
4)含氧空位AgIO3光催化剂的制备方法简易、快捷且绿色环保,具有广阔的应用前景。
附图说明
图1为实施例1中含氧空位AgIO3光催化剂的X射线衍射图;
图2为光催化剂的SEM图:(a)AgIO3;(b)AgIO3-Ov-3;
图3为光催化剂的TEM图:(a)AgIO3;(b)AgIO3-Ov-3;
图4为不同光催化剂在自然光照射下对甲基橙的降解曲线;
图5为不同光催化剂在自然光照射下降解甲基橙的表观速率常数,a-h分别为AgIO3-Ov-1,AgIO3-Ov-2,AgIO3-Ov-3,AgIO3-Ov-4,AgIO3-Ov-5,AgIO3-Ov-6和AgIO3-Ov-7;
图6为AgIO3-Ov-3光催化剂在自然光照射下对(a)盐酸四环素、(b)罗丹明B、(c)盐酸金霉素、(d)氧氟沙星、(e)磺胺异恶唑、(f)诺氟沙星和(g)甲基橙有机污染物的降解吸收全谱图及降解率图。
具体实施方式
下面将结合本发明的实施例中的附图,对本发明的实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
含氧空位AgIO3光催化剂的制备方法:
(1)AgIO3的制备:将0.1699 g硝酸银和0.1669 g五氧化二碘分别溶解于15 mL去离子水中,进行磁力搅拌处理,溶解完全后,分别得到均匀的硝酸银水溶液和五氧化二碘水溶液;在磁力搅拌条件下,将五氧化二碘水溶液缓慢滴入硝酸银水溶液中,反应液中硝酸银:五氧化二碘的摩尔比为2:1;在室温下搅拌反应2 h,反应结束后,所得产物经离心、去离子水洗涤、烘干后,得到AgIO3;
(2)含氧空位AgIO3光催化剂的制备:将0.2828 g步骤(1)所得的AgIO3加入坩埚中,然后将坩埚放入管式炉内,以5 ℃/min的升温速率加热升温至300 ℃,保温30 min;反应结束后自然冷却,所得产物经研磨后,得到含氧空位AgIO3光催化剂。
步骤(2)中AgIO3的质量为0.2 g,分别在100 ℃,200 ℃,300 ℃,400 ℃下烧结并保温30 min,在300 ℃下烧结分别保温15 min,30 min,60 min,120 min,得到AgIO3-Ov-1,AgIO3-Ov-2,AgIO3-Ov-3,AgIO3-Ov-4,AgIO3-Ov-5,AgIO3-Ov-6和AgIO3-Ov-7光催化剂。
所得复合光催化剂的XRD图见图1,SEM图见图2。通过制得样品的XRD图(图1)可以看出,含氧空位AgIO3光催化剂的所有的衍射峰位置都分别对应AgIO3的峰,并且无任何杂质峰,说明所制备出的含氧空位AgIO3光催化剂纯度高,结晶性较好。通过图2与图3中(a)AgIO3和(b)AgIO3-Ov-3的SEM图和TEM图对比,可以看出,上述方法制备的AgIO3光催化剂为片状,AgIO3-Ov-3光催化剂为块状。而AgIO3-Ov-3光催化剂的TEM图中非晶相区域(红色虚线)则代表损失的氧。
实施例2
将实施例1所得烧结光催化剂用于降解污染物实验。
实验步骤:通过在自然光下降解多种污染物水溶液对样品的光催化性能进行评估。首先将50 mg的催化剂分别加到装有40 mL的污染物水溶液(浓度为10 mg/L)的50 ml烧杯中, 然后烧杯在黑暗条件下搅拌0.5 h,使催化剂和目标降解物之间达到吸附-脱附平衡。之后将烧杯转移到室外太阳光下进行光照,每隔10 min用塑料吸管吸取3 mL液体,经离心机进行离心分离后取上层清夜,用分光光度计测定污染物水溶液的吸光度。
光催化降解率公式为:
D % = (C0-C)/ C0×100% = (A0-A)/ A0×100%
式中C0为目标降解物处理前初始浓度;C为目标降解物经过光催化处理后的浓度;A0为目标降解物处理前初始吸光度;A为目标降解物经过光催化处理后的吸光度。
将实施例1所得AgIO3-Ov-1,AgIO3-Ov-2,AgIO3-Ov-3,AgIO3-Ov-4,AgIO3-Ov-5,AgIO3-Ov-6和AgIO3-Ov-7共七种光催化剂用于催化甲基橙的降解,降解曲线如图4所示、降解过程的表观速率常数如图5所示。由图4可知,7种复合光催化剂的降解率分别为27%,35%,77%,36%,60%,69%和68%。其中,AgIO3-Ov-3光催化剂对甲基橙的降解率最高,可以达到77%。
将实施例1所得AgIO3-Ov-3光催化剂对甲基橙进行光催化降解后,污染物由原来的淡黄色几乎变为无色。
实施例3
将实施例1所得AgIO3-Ov-3光催化剂在自然光照射下对盐酸四环素、罗丹明B、盐酸金霉素、氧氟沙星、磺胺异恶唑、诺氟沙星和甲基橙等有机污染物进行光催化降解,降解吸收全谱图及降解率图如图6所示,该催化剂对七种有机污染物的降解率分别为71.5%,67.7%,71.2%,80.5%,30.4%,49.3%,77.1%,说明本发明对催化有机污染物的降解具有较好地普适性。
对比例1
按照实施例1中步骤(1)的方法制备得到AgIO3,SEM图见图2中(a),可以看出,AgIO3平均粒径尺寸约为0.5~3 μm。并将其用于催化降解甲基橙的实验,步骤同实施例2,降解率为18.0%,远低于AgIO3-Ov-3光催化剂。
对比例2
按照实施例1中步骤(1)的方法制备得到AgIO3,并将其在不同温度和不同时间下进行烧结,分别得到AgIO3-Ov-1,AgIO3-Ov-2,AgIO3-Ov-4,AgIO3-Ov-5,AgIO3-Ov-6和AgIO3-Ov-7然后用于光催化降解甲基橙的实验,步骤同实施例2,降解率分别为27%,35%,36%,60%,69%和68%,远低于AgIO3-Ov-3光催化剂。
最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (9)
1.一种含氧空位AgIO3光催化剂的制备方法,其特征在于,包括以下步骤:
S1、将AgIO3粉末称好放置在坩埚中;
S2、将坩埚放入管式炉中加热升温,待温度升至300 ℃,保温30min;
S3、反应结束后冷却,所得产物经过研磨后,得到AgIO3-Ov-3光催化剂。
2.根据权利要求1所述的一种含氧空位AgIO3光催化剂的制备方法,其特征在于,步骤S1中所述AgIO3的制备方法为:将硝酸银和五氧化二碘分别溶于15 ml超纯水中,将五氧化二碘水溶液缓慢滴入硝酸银水溶液中,在室温下搅拌反应2 h,反应结束后,所得产物经离心、洗涤、烘干后,得到AgIO3。
3.根据权利要求2所述的一种AgIO3光催化剂的制备方法,其特征在于,所述硝酸银:五氧化二碘的摩尔比为2:1。
4.根据权利要求1所述的一种含氧空位AgIO3光催化剂的制备方法,其特征在于,步骤S1中所述AgIO3粉末的粒径为0.5~3 μm。
5.根据权利要求1所述的一种含氧空位AgIO3光催化剂的制备方法,其特征在于,步骤S1中所述AgIO3粉末称量为0.2 g。
6.根据权利要求1所述的一种含氧空位AgIO3光催化剂的制备方法,其特征在于,步骤S2中所述加热升温的升温速率为5 ℃/min。
7.根据权利要求1所述的一种含氧空位AgIO3光催化剂的制备方法,其特征在于,步骤S3中所述冷却为自然冷却。
8.一种含氧空位AgIO3光催化剂,其特征在于,根据权利要求1~7中任一项所述的制备方法制得。
9.根据权利要求8所述的一种含氧空位AgIO3光催化剂,其特征在于,在光催化降解有机染料方面的应用。
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